Home Crystal structure of 2,2′-((((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))bis(azanylylidene))bis(methanylylidene))diphenolato-κ2N;κ4O)nickel(II), C28H22N2O4Ni
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Crystal structure of 2,2′-((((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))bis(azanylylidene))bis(methanylylidene))diphenolato-κ2N4O)nickel(II), C28H22N2O4Ni

  • Qiang Xu , Yan Ling Zhao , Xiao Fang Luo , Ming Wei Zhou and Guo qiang Li EMAIL logo
Published/Copyright: March 5, 2018

Abstract

C28H22N2NiO4, tetragonal, P41212 (no. 92), a = 10.989(4) Å, c = 18.470(2) Å, V = 2230.4(16) Å3, Z = 4, Rgt(F) = 0.0571, wRref(F2) = 0.1382, T = 293(2) K.

CCDC no.: 1419886

The crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Red block
Size:0.26 × 0.21 × 0.19 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:0.91 mm−1
Diffractometer, scan mode:Bruker APEX-II, φ and ω-scans
θmax, completeness:27.5°, >99%
N(hkl)measured, N(hkl)unique, Rint:13577, 2556, 0.155
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1372
N(param)refined:160
Programs:Bruker programs [1], SHELX [2, 3] , OLEX2 [4]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
N10.1734(5)0.3941(5)0.0556(3)0.0427(14)
Ni10.29264(8)0.29264(8)0.0000000.0461(4)
O10.3216(5)0.4203(4)−0.0736(2)0.0560(14)
O20.2028(4)0.1515(4)0.0721(2)0.0505(12)
C10.2700(7)0.5281(6)−0.0765(4)0.0506(19)
C20.2973(8)0.6058(7)−0.1349(3)0.0565(19)
H20.3495260.578063−0.1709460.068*
C30.2496(7)0.7210(8)−0.1409(4)0.067(2)
H30.2707020.769176−0.1803200.081*
C40.1713(8)0.7663(7)−0.0895(4)0.077(3)
H40.1406280.844916−0.0934100.092*
C50.1389(8)0.6928(7)−0.0320(4)0.067(2)
H50.0852880.7229870.0025760.081*
C60.1848(6)0.5721(6)−0.0238(4)0.0464(18)
C70.1463(6)0.5068(6)0.0385(4)0.0465(18)
H70.0963200.5484750.0707240.056*
C80.1248(6)0.3401(6)0.1190(4)0.0460(18)
C90.0677(7)0.4010(7)0.1768(4)0.059(2)
H90.0621300.4854140.1758760.071*
C100.0201(7)0.3382(7)0.2345(4)0.064(2)
H10−0.0157310.3807750.2723800.076*
C110.0247(6)0.2123(8)0.2370(4)0.0556(18)
H11−0.0115010.1708240.2752960.067*
C120.0830(6)0.1483(7)0.1828(4)0.051(2)
H120.0876860.0638570.1846030.061*
C130.1349(6)0.2126(7)0.1251(3)0.0444(16)
C140.1350(8)0.0671(6)0.0287(4)0.061(2)
H14A0.0781940.0225280.0588900.073*
H14B0.1899580.0090610.0063830.073*

Source of material

N,N′-bis(salicylaldehyde)-1,4-bis(o-aminophenoxy)ethane (H2L) used in the present work was synthesized via a standard Schiff base condensation reaction of salicylaldehyde (0.977 g, 8 mmol) and bis(4-aminophenoxy)ethane (0.977 g, 4 mmol) following a literature procedure [5]. All other reagents were purchased from Shanghai Aladdin Biochem (China) and used without further purification. A mixture of Ni(ClO4)2⋅6H2O (36.6 mg, 0.1 mmol) and H2L (45.3 mg, 0.1 mmol) in 30 mL MeOH/dichloromethane (1:2, v/v) was stirred at ambient temperature for 30 min to afford a claybank solution. The mixture was filtered and the filtrate was shelved in a sealed bottle filled with diethyl ether atmosphere, and the well-shaped reddish crystals were obtained in a yield of 42% (based on Ni).

Experimental details

The structure is also refinable in the entiomorphic chiral space group P43212 as an inversion twin. All of the hydrogen atoms were placed in the calculated positions and all the non-hydrogen atoms were refined anisotropically.

Discussion

Over the last few decades the design and synthesis of Salen-type schiff base complexes were studied because of their fascinating structure and potential properties [6], [7], [8]. Some schiff base complexes are similar to bio-enzyme systems and suitable for the simulation of bioscience [9], [10]. Moreover, nickel is one of the essential trace elements in organisms, which can promote absorption of iron, growth of red blood cells, synthesis of aminase and may be also a kind of structural stabilizer for DNA and RNA [11].

The Ni(II) center is six-coordinated by two nitrogen and four oxygen atoms from the hexadentate Salen-type L2− dianion to form two six-membered and three five-membered rings and exhibits a slightly distored-octahedral geometry. The axial positions are occupied by two imine nitrogen (N1) atoms with the Ni—N bond lengths of 2.004(5) Å, and the N1—Ni—N1 bond angle is 172.1(3)°. The equatorial plane are defined by two phenolic oxygen atoms (O1) and two ether oxygen atoms (O2) with the Ni—O distance of 1.979(5) Å and 2.270(5) Å, and the bond angles around the Ni(II) atom vary from 75.5(2)° to 163.14(19)°.

Acknowledgements

We acknowledge support for the publication fee by the Scientific Research Fund of Chongqing Municipal Education Commissionthe (KJ1601115), Chongqing University of Arts and Sciences (Z2015CH02), Chongqing University of Arts and Sciences (XSKY2017036), Chongqing University of Arts and Sciences (XSKY2017037).

References

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Received: 2017-11-9
Accepted: 2018-2-20
Published Online: 2018-3-5
Published in Print: 2018-5-24

©2018 Qiang Xu et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

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